Process of clarifying and deodorizing oil-of-wood turpentine.



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f UNrrijnsTA'riis PATENT @FFIGE.

Specification of Letters Patent.

Patented Sept. 4, 1906.

Application filed May 26, 1906. Serial No. 318,832.

To all whmn it may concern.-

Be it known that I, EDUARD HEBER, doctor of philosophy, a subject of the German Emperor, residing at No. 107 Henry street, in the city of New York, borough of Brooklyn, county of Kings, and State of New York, have invented a certain new and useful Process for Clarifying and Deodorizing Oil-ofiVood Turpentine, of which the following is a specification.

This invention relates to the process for clarifying and deodorizing oil-of-wood turpentine, and has for its object to render the process more expeditious and considerably cheaper.

Oil-of-wood turpentine in the United States is obtained from the roots and trunks of the dead long-leaf pine (Pines maritime) and is ordinarily obtained from the light wood or heart from which the outer covering ofsap ivood has been rotted away. It is ordinarily obtained by heating the wood in a suitable retort in which the oil-of-wood turpentine is vaporized, and afterward it is condensed and collected. As thus obtained it consists not only of oil-of-wood turpentine, but also coloring-matter, odoriferous matter, and tarry substances.

My process of purification is as follows: I first remove the tarry constituents by distillation over lime. This is accomplished by mixing the crude oil-ofwood turpentine thoroughly with from one to two per cent. of lime mixed with water and then distilling by means of steam. The oil-of-wood turpentine is then mechanically separated from the water, and as thus obtained it is in a partially purified and clarified condition, but still contains considerable coloring and odorifcrous matter. Then I add to the oilof-wood turpentine a suflicient quantity of ordinary soap solution to dissolve or emulsify the oil and then treat this oil-of-wood-turpentine solution or emulsion with potassium permanganate, sodium permanganate, or calcium permanganate mixed with sulfuric acid. Soap solution possesses the property of dis solving or emulsifying oil-of-wood turpentine, the result being that when the potassium permanganate and sulfuric acid are mingled with the emulsified oil-of-wood turpentine these chemicals come into contact with all the minute particles thereof and practically with all the particles at once. It is not possible to accomplish the same result with an agitator alone, for the reason that the oil-ofwood turpentine, which must be mingled with water, cannot by the best-known agitator be broken up into particles sufliciently small to enable the operator to accomplish the same result. As a result of the emulsification the permanganate is in a position to readily destroy only the odoriferous matter and the coloringanatter of the oil-of-wood turpentine, which, as I have discovered, are more easily oxidized or attacked than the oilof-wood turpentine, and this result is accomplished without the destruction of any appreciable part of the pure oil-ofwood turpentine. I am thus able to accomplish the desired result with a minimum amount of chemicals and with the destruction of a minimum amount of oil-of-wood turpentine, and I am also able to more thoroughly deodorize and clarify my product.

An example of my process is as follows: I place one hundred pounds of oilofwood turpentine from which the tarry constituents have been removed by distillation over lime,

as above described, in an ordinary iron still or retort which is provided with a suitable agitator. To this I add a sufficient quantity of ten-per-cent. soap solution to thoroughly dissolve or emulsify the oil-of-wood turpentine. Into this emulsion I flow slowly a fiveper cent. permanganate solution holding three to live pounds of potassium permanganate and four to six pounds of concentrated sulfuric acid of 66 Baum in solution while the contents of the still'is being constantly agitated or stirred. The agitation is continued until the permanganate solution introduced into the still has completely lost its color, after which by the addition of calcium chlorid or zinc sulfate the soap solution is precipitated as indissoluble calcium or zinc soap. The oil-of-wood turpentine is then distilled off by means of steam or high-pressure steam, after which the oil-ol-wood turpentine is mechanically separated from the water and forms a colorless liquid having an agreeable odor resembling that of essential oils and very similar to gum-turpentine. The treatment with. chromic acid and sulfuric acid. may be effected in the same manner, the same proportions and the same strength of solution being used as when the treatment is with potassium permanganate, described above, the stirring of the mixture being continued until the change of color of the chromic acid indicates that the reaction has been completed. If chromic acid is emor emulsified by a soap solution, as above deployed in the shape of its salts, about six to 1 nine pounds of potassium bichromate (or a corresponding quantity of sodium bichromate) should be used for each one hundred pounds of oil-of-wood turpentine, which has been subjected to a preliminary purification by distillation over lime, and then dissolved scribed. These six to nine pounds of bichromate are converted into a fiveper-cent. aqueous solution, and four to seven pounds of concentrated sulfuric acid of 66 Baum are added to the same. The solution thus prepared is caused to flow slowly into the still, as above described, and the operation is completed exactly as described for chromic acid.

Having thus described my process, what I claim is 1. The process of clarifying and deodorizing oil-of-woo'd turpentine, which consists of first emulsifying the oil-of-wood turpentine with a soap solution, and then adding to the same chemicals, which attack and destroy the coloring-matter and odoriferous matter mingled therewith.

2. The process of clarifying and deodorizing oil-of-wood turpentine, which consists of emulsifying the oil-of-wood turpentine with a soap solution, adding thereto chemicals which will attack and oxidize the coloringmatter and odoriferous matter mingled therewith, precipitating the soap solution, and

separating the oil-ofwood turpentine therefrom.

3. The process of clarifying and deodorizing oil-of-wood turpentine, which consists in first removing the tarry substances by distillation over lime, emulsifying the oil-of-wood turpentine, adding thereto chemicals which will attack and oxidize the odoriferous matter and coloring-matter mingled therewith, precipitating the soap solution and separating the oil-of-wood turpentine therefrom.

4. The process of deo'dorizing and clarifying oil-of-wood turpentine, which consists of first removing the tarry substances by distillation over lime, second, emulsifying the resultant product with a soap solution, third, adding to the emulsion chemicals which will attack and oxidize or destroy the odoriferous matter and coloring-matter which are mingled with the oil-of-wood turpentine, fourth, precipitating the soap solution, and fifth, distilling off the oil-of-wood turpentine by means of steam, condensing the same, and separating the oil-of-wood turpentine from the water by any mechanical means.

Signed at New York city, in the county of New York and State of New York, this 21st day of May, A. D. 1906.

EDUARD HEBER. l/Vitnesses:

D. P. Fos'rER, B. A. ITTNER. 

